文献类型：期刊文献

中文题名：阻燃剂乙基膦酸二乙酯(DEEP)的合成新方法及结构表征

英文题名：New method for synthesis and structural characterization of flame retardant diethyl ethylphosphonate(DEEP)

作者：张猛[1,2] 周永红[1,2] 胡立红[1,2] 李书龙[1,2] 刘红军[1,2] 曹振华[2]

第一作者：张猛

机构：[1]中国林业科学研究院林产化学工业研究所,国家林业局林产化学工程重点开放性实验室,江苏南京210042;[2]江苏强林生物能源有限公司,江苏溧阳213364

年份：2010

卷号：32

期号：8

起止页码：721-724

中文期刊名：化学试剂

外文期刊名：Chemical Reagents

收录：CSTPCD;;北大核心:【北大核心2008】；CSCD:【CSCD2011_2012】；

基金：国家林业局“948”项目(2009-4-55);国家重大产业技术开发专项项目(发改高技[2008]2441号);常州市科技攻关项目(CE2008075)

语种：中文

中文关键词：乙基膦酸二乙酯(DEEP);Michaelis-Arbuzov反应;微波

外文关键词：diethyl ethylphosphonate（DEEP）; Michaelis-Arbuzov reaction; microwave

分类号：TQ314

摘要：采用未见文献报道的烷基化试剂对甲基苯磺酸乙酯通过Michaelis-Arbuzov重排反应合成标题化合物,反应结束后烷基化试剂易于分离且可以重复使用;较目前工业所用烷基化试剂成本大大降低。采用常规和微波两种方法合成了标题化合物,分别考察了反应时间、烷基化试剂用量、微波功率对产率的影响,其中微波产率高达95.2%;最后通过GC、FT-IR、MS、HNMR对产物含量和结构进行了分析。
The flame retardant diethyl ethylphosphonate was synthesized by the Michaelis-Arbuzov rearrangement using ethyl p-toluenesulfonate as the alkylating agent,which has not been reported yet in the literature.The alkylating agent was separated easily from the product after reaction and could be reused,and the production cost was greatly reduced compared to the currently used commercial alkylating agents.In this paper,two methods including the conventional and microwave methods were used to synthesize the target compound DEEP,respectively.The effects of reaction time,amount of alkylating agent,and the microwave power on the product yield were described,with the maximum yield of microwave method reaching 95.2%.Finally,the content and structure of the product were analyzed by GC,FT-IR,MS,and 1HNMR.